Water → HCID 11166752、化合物

HRID 378911ノート

反応式

HRID 378911 の反応式
[CH3:1][O:2][CH2:3][CH2:4][OH:5].[H-].[Na+].Cl[C:9]1[N:10]=[C:11]([N:26]2[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]2)[C:12]2[N:17]=[C:16](Cl)[N:15]=[C:14]([N:19]3[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]3)[C:13]=2[N:25]=1.[OH2:32]>C1COCC1>[CH3:1][O:2][CH2:3][CH2:4][O:5][C:9]1[N:10]=[C:11]([N:26]2[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27]2)[C:12]2[N:17]=[C:16]([O:32][CH2:4][CH2:3][O:2][CH3:1])[N:15]=[C:14]([N:19]3[CH2:24][CH2:23][CH2:22][CH2:21][CH2:20]3)[C:13]=2[N:25]=1

参加物

6

反応物 4

HCID 962WaterHCID 80192-MethoxyethanolHCID 24758Sodium hydrideHCID 815562,6-Dichloro-4,8-di(piperidin-1-yl)pyrimido(5,4-d)pyrimidine

生成物 1

HCID 11166752HCID 11166752、化合物収率 34%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

2-Methoxyethanol (0.38 g, 5 mmol) was dissolved in dry THF (5 ml) and added to sodium hydride (0.12 g, 5 mmol) and stirred for 8 hours at room temperature. 2,6-dichloro-4,8-dipiperidinopyrimidopyrimidine (0.184 g, 0.5 mmol) in dry THF (10 ml) was added to this and the mixture heated under reflux for 32 hours. After cooling to room temperature, water (30 ml) was added and the product extracted into ethyl acetate (4×20 ml), the organic layers combined, dried (MgSO4), filtered and the solvent removed in vacuo. Recrystallisation from methanol/water yielded the title compound as a white solid (0.076 g, 34%), m.p. 127-128° C. Found C, 59.31; H, 7.60; N, 18.80. C22H34N6O4 requires C, 59.17; H, 7.67; N, 18.82%.

後処理

  1. temperatureheated
  2. temperatureunder reflux for 32 hours
  3. temperatureAfter cooling to room temperature
  4. extractionthe product extracted into ethyl acetate (4×20 ml)
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customthe solvent removed in vacuo
  8. customRecrystallisation from methanol/water

出典と根拠

ORDレコード
ord-71d9e201483b4ba58813d3660bc4204a
出典データセット
uspto-grants-2001_10
特許番号
US06297250B1

反応ノート

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